US6472632B1 - Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder - Google Patents
Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder Download PDFInfo
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- US6472632B1 US6472632B1 US09/396,046 US39604699A US6472632B1 US 6472632 B1 US6472632 B1 US 6472632B1 US 39604699 A US39604699 A US 39604699A US 6472632 B1 US6472632 B1 US 6472632B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
- C01F7/422—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation with a gaseous oxidator at a high temperature
- C01F7/424—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation with a gaseous oxidator at a high temperature using a plasma
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/48—Generating plasma using an arc
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0809—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes employing two or more electrodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0822—The electrode being consumed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0824—Details relating to the shape of the electrodes
- B01J2219/0826—Details relating to the shape of the electrodes essentially linear
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0824—Details relating to the shape of the electrodes
- B01J2219/0826—Details relating to the shape of the electrodes essentially linear
- B01J2219/083—Details relating to the shape of the electrodes essentially linear cylindrical
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0837—Details relating to the material of the electrodes
- B01J2219/0843—Ceramic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0845—Details relating to the type of discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0894—Processes carried out in the presence of a plasma
- B01J2219/0896—Cold plasma
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
- Y10S977/775—Nanosized powder or flake, e.g. nanosized catalyst
- Y10S977/776—Ceramic powder or flake
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/778—Nanostructure within specified host or matrix material, e.g. nanocomposite films
- Y10S977/786—Fluidic host/matrix containing nanomaterials
- Y10S977/787—Viscous fluid host/matrix containing nanomaterials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/84—Manufacture, treatment, or detection of nanostructure
- Y10S977/888—Shaping or removal of materials, e.g. etching
- Y10S977/889—Shaping or removal of materials, e.g. etching by laser ablation
Definitions
- the present invention generally relates to a method and system for the production of submicron materials, and more particularly to a method and system of synthesizing, in bulk quantities, nanosized powders, including nanocrystalline ceramics.
- Ceramic materials are used in a wide variety of applications, and generally have excellent heat resistance, corrosion resistance, and abrasion resistance, as well as unique electrical or optical properties. Ceramic material, as used herein, generally refers to an oxide, nitride, boride or carbide of a metal, or a mixture thereof. Very fine ceramic powders are used in a large number of industrial processes to introduce or modify material properties. These materials can pose difficulties in sintering but, when they are converted to ultrafine particles, particularly submicron crystalline particles, numerous traditional problems are avoided. Accordingly, several processes have been devised for fabricating ultrafine, or submicron, crystalline materials, such as those of 1-500 nanometer size, referred to herein as nanosized or nanocrystalline.
- sol-gel sol-gel
- Thermal processes create the supersaturated vapor in a variety of ways, including laser ablation, plasma torch synthesis, combustion flame, exploding wires, spark erosion, electron beam evaporation, sputtering (ion collision).
- laser ablation a high-energy pulsed laser is focused on a target containing the material to be processed.
- the high temperature of the resulting plasma greater than 10,000° K
- the process is capable of producing a variety of nanocrystalline ceramic powders on the laboratory scale, but it has the great disadvantage of being extremely expensive due to the inherent energy inefficiency of lasers, and so it not available on an industrial scale.
- the use of combustion flame and plasma torch to synthesize ceramic powders has advanced more toward commercialization.
- the precursor material can be a solid, liquid or gas prior to injection into the flame or torch, under ambient pressure conditions. (the most common precursor state is a solid material).
- the primary difference between the two processes is that the combustion flame involves the use of an oxidizing or reducing atmosphere, while the plasma torch uses an inert gas atmosphere.
- Each of these processes requires relatively expensive precursor chemicals, such as TiCl 4 for the production of TiO 2 by the flame process, or TiC and TiB 2 by the plasma process.
- a feature of both methods is the highly agglomerated state of the as-synthesized nanocrystalline ceramic powders.
- reactants are delivered to a plasma jet produced by a plasma torch. See generally, U.S. Pat. Nos. 4,642,207 and 5,486,675.
- the feed material may be delivered to the plasma stream by arc vaporization of the anode.
- the anode is normally metallic but may be a metal-ceramic composite.
- electrothermal gun electrothermal gun
- the electrogun is a pulsed power device which employs an electrode erosion phenomenon to vaporize one of the discharge electrodes (the cathode).
- the eroded metal vapor is subsequently ionized to form a dense plasma in which the high current discharge is sustained.
- the electrogun has a small length-to-diameter ratio and is designed to resist bore wall erosion.
- the vaporized metal exits the electrogun in a high-temperature, high-pressure, high-velocity jet. This jet is directed into a reactor filled with an appropriate atmosphere for reaction of the metal and quenching of the nanoparticles produced.
- the high-pressure jet expands rapidly. This expansion produces rapid cooling which promotes condensation of the vaporized material, thereby forming a spray of high-velocity metallic nanoparticles.
- the electrogun uses batch processing powered by high-energy current pulses, while a plasma torch which operates continuously. Electrothermal synthesis, unlike plasma torch, heats the feed material directly, and does not produce any waste stream of process gases.
- the use of an electrogun is still somewhat energy inefficient, however, since it is necessary to chemically react the raw material to produce the nanoparticles, as opposed to merely physically converting another form of the material. It would, therefore, be desirable to devise a method of synthesizing nanocrystalline ceramics which is more energy efficient, and suitable for an industrial scale. It would be further advantageous if the method could reduce material cost.
- a method of producing ceramic powder generally comprising the steps of creating a plasma stream in a reactor vessel, and physically converting a ceramic precursor material into ceramic particles suspended in the vessel, using the plasma stream.
- the plasma stream is directed into an atmosphere of the vessel whose ambient conditions are selected to yield nanocrystalline ceramics.
- a metallic reactant may additionally be introduced into the vessel using the plasma stream, wherein the metallic reactant forms ceramic particles having the same composition as the ceramic particles of the physical converting step.
- the plasma stream may be created by delivering electrical current to an electrothermal gun.
- the gun has a ceramic barrel which is eroded by the plasma stream.
- the ceramic precursor material is injected as particulates into the plasma stream, the ceramic precursor particulates having a first size (e.g., micron or larger), and the ceramic particles suspended in the vessel have a second size which is substantially smaller than the first size (e.g., nanosized).
- FIG. 1 is a schematic diagram of a system for electrothermal synthesis of nanocrystalline ceramics in accordance with one embodiment of the present invention
- FIG. 2 is a cross-sectional view of an electrothermal gun used with the system of FIG. 1;
- FIG. 3 is a pictorial representation of the synthesis of nanocrystalline ceramic powder using the system of FIG. 1;
- FIG. 4 is a cross-sectional view of an alternative electrothermal gun for use with the present invention.
- System 8 is generally comprised of a high-current electrical power supply 10 with heavy-duty wiring 12 for conducting an energetic current pulse, an arc initiator power supply 14 with wiring 16 , a ceramic electrothermal gun (electrogun) 18 with a cooling system 20 , a reactor atmosphere supply system 22 with a supply pipe 24 and atmosphere control system 26 , and a reactor vessel 28 having a reactor atmosphere 30 illustrated with suspended nanoparticles 32 , and a layer of settled nanopowder 34 on the floor of the vessel.
- a high-current electrical power supply 10 with heavy-duty wiring 12 for conducting an energetic current pulse
- an arc initiator power supply 14 with wiring 16
- a ceramic electrothermal gun (electrogun) 18 with a cooling system 20
- a reactor atmosphere supply system 22 with a supply pipe 24 and atmosphere control system 26
- a reactor vessel 28 having a reactor atmosphere 30 illustrated with suspended nanoparticles 32 , and a layer of settled nanopowder 34 on the floor of the vessel.
- power supply 10 provides pulsed current to electrogun 18 in concert with initiation of an arc by initiator power supply 14 , which results in activation of electrogun 18 .
- a plasma stream from electrogun 18 entrains raw metal precursor material and ceramic precursor material which become vaporized in reactor vessel 28 , and subsequently condense as nanocrystalline particles 32 .
- electrogun 18 may be constructed in a fashion similar to conventional electrothermal guns (such as those used for spacecraft thrusters, the production of railgun plasma armatures, or the ignition of propellants to accelerate projectiles in guns), except that electrogun 18 is provided with a ceramic barrel, that is, a barrel whose material is the same (chemically, although not in the same physical state) as the nanopowder which is desired to be produced.
- electrothermal guns such as those used for spacecraft thrusters, the production of railgun plasma armatures, or the ignition of propellants to accelerate projectiles in guns
- electrogun 18 includes a cathode 40 , a non-eroding anode 42 , a structural shell or housing 44 with coolant channels 60 , a ceramic liner 46 forming the gun barrel, a muzzle seal 48 , a breech seal 50 , and arc initiator lines 52 .
- the material of ceramic liner 46 is specifically selected to erode during generation of the plasma stream within the bore of electrogun 18 .
- the synthesis process thus preferably includes the generation of nanosized particles from both (1) the reaction of the metallic (or organometallic) cathode 40 , and (2) the physical conversion of the material of ceramic liner 46 to a nanosized form as a result of the gun blast.
- electrogun 18 has a length-to-diameter ratio of at least ten.
- the synthesis process is illustrated further in FIG. 3 .
- Power is supplied to cathode/anode pair 40 / 42 via power supply 10 while an electric arc is established via initiator lines 52 .
- the high-current electric arc 80 passes between cathode 40 and anode 42 , and a high-pressure, high-velocity, high-temperature stream of plasma 82 flows down the bore of electrogun 18 .
- Ceramic material 47 is ablated from ceramic liner 46 , and become entrained in plasma stream 82 . Particles thus entrained lose mass through vaporization, and become smaller or vaporize completely.
- Reactant material 39 from cathode 40 also becomes entrained in plasma stream 82 .
- the high-pressure plasma exits the confines of electrogun 18 , it undergoes rapid isotropic expansion.
- rapid expansion is a rapid cooling.
- the cooled plasma then condenses into a high-velocity spray of extremely fine (nanosize) ceramic particles 84 .
- the energetic expansion produces turbulent mixing of the condensed droplets or particles with the reactor atmosphere 83 .
- Any metallic particles 86 produced by electrode erosion or by disassociation of ceramic quickly react with the reactor atmosphere 83 , forming ceramic particles 84 .
- a suspension of nanoparticles is produced, which gradually settle to the floor of the reactor vessel where they may be collected.
- the reactor atmosphere serves two primary purposes, to react any metal particles which may be mixed in with the ceramic particles, and to rapidly quench the ceramic particles, since unquenched particles would tend to bond tightly together or even grow together into a single particle. Quenched particles may stick together, but more loosely than hot particles. Quenched particles do not tend to grow into a single particle.
- the electrothermal synthesis taught herein provides a method for the direct and efficient conversion of ceramic material into ceramic nanopowder, thereby realizing a material cost saving in comparison to competing methods. Energy costs are also reduced inasmuch as the ceramic feed material is heated directly rather than indirectly as is the case of prior art plasma torch processes.
- the present invention unlike plasma torch processes, requires no working gas. There is no mixing of gas streams, and no circulation of the reactor atmosphere through the plasma arc, and further there is no need to use a refrigerated quenching surface. Reactions go to completion in less than a millisecond.
- the technique has proven particularly suitable for production of titanium and aluminum oxide and nitride. No byproducts are produced, and the process is well-suited for automation.
- FIG. 4 illustrates an alternative embodiment for an electrogun 70 which may be used with the present invention.
- Electrogun 70 has a conical, rather than cylindrical, bore. Additionally, a ceramic insert 72 having a cylindrical body 74 and a conical tip 76 is advanced into the bore. The conical bore and conical tip 76 form a divergent annular passageway. Ceramic material which is to be physically converted to nanopowder is extracted from both the ceramic bore liner and insert 72 . In this manner, the insert is easily changed when it as been consumed (i.e., it is used for more than one shot of electrogun 70 ). The replacement of insert 72 is particularly advantageous since it is more easily eroded that the bore liner, and the liner is less conveniently replaced.
- the cross-sectional area of the annular passageway is easily adjusted by changing the axial (longitudinal) position of the insert, so simple adjustments compensate for erosion of the conical bore liner as well (to maintain a particular passageway cross-section). Erosion of the passageway is actually self-adjusting, since erosion will be greater where the passageway is smaller, and vice-versa.
- Physical properties of the insert can be adjusted to favor erosion of the insert. For example, it can be made relatively porous.
- the ceramic precursor material may be injected as particulates into the plasma stream, wherein the ceramic precursor particulates have a first size (e.g., micron or larger), and the ceramic particles suspended in the vessel have a second size which is substantially smaller than the first size (e.g., nanosized).
- the precursor material would preferably be injected radially in the breech region, allowing sufficient residence time within the gun.
- the injection technique may be combined with the above-described technique using the ceramic liner 46 which erodes during generation of the plasma stream.
- the muzzle electrode 42 has a cylindrical bore with a rectangular cross-sectional profile.
- the inner diameter of the bore of muzzle electrode 42 is substantially flush (e.g., radially aligned and axially aligned) with the inner diameter of barrel 46 .
- This geometry contiguously extends an axial length of the cylindrical barrel 46 by an axial dimension of the bore of muzzle electrode 42 .
- other gun geometries might be used. It is therefore contemplated that such modifications can be made without departing from the spirit or scope of the present invention as defined in the appended claims.
Abstract
Description
Claims (16)
Priority Applications (9)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/396,046 US6472632B1 (en) | 1999-09-15 | 1999-09-15 | Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder |
US09/661,330 US6600127B1 (en) | 1999-09-15 | 2000-09-13 | Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder |
JP2001524399A JP2003509229A (en) | 1999-09-15 | 2000-09-14 | Method and apparatus for mass production of nano-sized materials by electrothermal gun synthesis |
PCT/US2000/025163 WO2001020953A1 (en) | 1999-09-15 | 2000-09-14 | Method and apparatus for producing bulk quantities of nano-sized materials by electrothermal gun synthesis |
EP00968356A EP1216605A1 (en) | 1999-09-15 | 2000-09-14 | Method and apparatus for producing bulk quantities of nano-sized materials by electrothermal gun synthesis |
CA002382107A CA2382107A1 (en) | 1999-09-15 | 2000-09-14 | Method and apparatus for producing bulk quantities of nano-sized materials by electrothermal gun synthesis |
IL14812400A IL148124A0 (en) | 1999-09-15 | 2000-09-14 | Method and apparatus for producing bulk quantities of nano-sized materials by electrothermal gun synthesis |
US09/695,465 US6653591B1 (en) | 1999-09-15 | 2000-10-24 | Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder |
US10/023,685 US6580051B2 (en) | 1999-09-15 | 2001-12-18 | Method and apparatus for producing bulk quantities of nano-sized materials by electrothermal gun synthesis |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US09/396,046 US6472632B1 (en) | 1999-09-15 | 1999-09-15 | Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
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US09/661,330 Continuation-In-Part US6600127B1 (en) | 1999-09-15 | 2000-09-13 | Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder |
US09/695,465 Division US6653591B1 (en) | 1999-09-15 | 2000-10-24 | Method and apparatus for direct electrothermal-physical conversion of ceramic into nanopowder |
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US6472632B1 true US6472632B1 (en) | 2002-10-29 |
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